液相色谱-电喷雾电离质谱法检测地高辛人血浆药物浓度方法学的建立与考证

Development and validation of a liquid chromatographic/electrospray ionization mass spectrometric method for the determination of digoxin in human plasma

目的:建立适用于地高辛临床血药浓度监测的液相色谱-电喷雾电离质谱方法(LC-ESI-MS)。方法:地高辛人血浆样本采用乙酸乙酯液液萃取后以LC-ESI-MS方法进行分析。采用Kro-masilC18柱(150mm×2.00mm,3.5μm)分析柱;在乙腈和氯化铵的混合流动相的流动相系统中,进行梯度洗脱,选择性负离子检测,地高辛m/z为815.40,内标Rg2m/z为819.00。结果:地高辛在0.05～10.0ng/mL浓度范围内线性关系良好(r=0.9989),血浆内杂质不影响药物的检测,方法回收率大于75%,批内、批间变异均小于15%,冻融稳定性良好。结论:本研究所建立的LC-ESI-MS测定方法操作简便、快速、灵敏,准确,重现性好,所需血浆量少,可用于地高辛临床血药浓度监测及临床药动学研究。

AIM:To develop a sensitive and selective liquid chromatography-electrospray ionization mass spectrometry(LC-ESI-MS)method for clinical identification and quantification of digoxin in human plasma.METHODS:The method was based on simple liquid-liquid extraction(LLE).A Kromasil C18 column(150 mm×2.00 mm,3.5 μm)was used as the analytical column,while a mixture of acetonitrile and 500 μmol/L ammonium chloride was used as the mobile phase.MS detection was performed using a single quadrupole mass spectrometer in a...